Effects of Na_2SiF_6 on Preparing Mullite Material with Sludge from the Aluminum Profile Factory and Pyrophyllite

In this research,the mullite material with sludge from aluminum profile factory and pyrophyllite as primary raw materials was prepared. Based on the optimal formula,optimal calcining temperature and holding time determined in the research,effects of Na2SiF6 mineralizer on crystal structure,microstructure and properties of mullite were discussed to determine the optimal addition of Na2SiF6 mineralizer. With XRD and SEM methods,crystal structure and microstructure of the test samples were characterized; with Rietveld Quantification method,contents of various crystal phases in the test samples were determined; properties of the test samples were tested. In combination with the structural and property analysis results,the optimal Na2SiF6 addition was determined to be 2%. Correspondingly,the content of solid solution of mullite-Al4.59Si1.41O9.7 was 96.9wt%,the bulk density was 2.10 g/cm3,the degree of porosity was 27.0%,the water absorption rate was 12.8%,the rupture strength was 24.30 MPa and primary thermal-shock rupture strength retention rate was 87.4%.

Synthesis,Crystal Structure and Antimicrobial Activity of a New Ternary Copper(Ⅱ) Complex with p-Chlorophenoxyacetic Acid and 2-Amino Benzothiazole

A novel ternary complex of Cu（pcpa）2（aben）2 （pcpa=p-chlorophenoxyacetic acid anion,aben=2-amino benzothiazole） was synthesized by the reaction of copper acetate,2-amino benzothiazole and p-chlorophenoxyacetic acid.Elemental analysis,IR,UV and X-ray single-crystal diffraction were carried out to determine the composition and crystal structure.The crystal crystalli-zes in the monoclinic system,space group C2/c with a=25.795（4）,b=7.384（3）,c =17.741（6）,β=107.47（2）°,C30H24Cl2CuN4O6S2,Mr=735.09,V=3223.2（18） 3,Z=4,Dc=1.515 Mg/m3,λ（MoKα）=0.71073 ,μ=1.022 mm-1,F（000）=1500,the final R=0.0464 and wR=0.1244.A total of 3218 unique reflections were collected,of which 2228 with I 〉 2σ（I） were observed.The Cu（II） atom is four-coordinated with two carboxylate oxygen atoms of the two pcpa ligands and two nitrogen atoms in thiazole rings of two aben ligands.The analysis of crystal structure shows intermolecular and intramolecular hydrogen bonds between amino-nitrogen atoms of the two aben ligands and carboxylate oxygen atoms of the two pcpa ligands.The antimicrobial properties of the title complex and its two free ligands were tested against representative bacterial and fungal strains.Results show that the antibacterial activity of the complex is less than or equal to that of 2-amino benzothiazole,but for yeasts and moulds,it exhibits excellent inhibitory effect better than that of its two free ligands.

Synthesis and Crystal Structure of 3-Benzyl-6-trichloromethyl-[1,2,4] triazolo[3,4-b][1,3,4]thiadiazole

The title compound 3-benzyl-6-trichloromethyl-[1,2,4]triazolo[3,4-b][1,3,4]thiadiazole I （C11HTC13N4S, Mr = 333.62） has been synthesized, and its structure was determined by elemental analyses, IR, ^1H NMR, ^13C NMR, and X-ray diffractions. The crystal is of triclinic, space group P1^-, with a = 5.898（3）, b = 10.510（4）, c = 11.580（5） A, α = 74.936（7）, β= 75.476（7）, γ = 79.647（7）°, V= 665.9（5）/A^3, F（000） = 336, Z= 2, Dc = 1.664 g/cm^3, 2 = 0.71073A, p = 0.834 mm^-1, the final R = 0.0605 and wR = 0.0900. The secondary bonding interactions （SBIs） S…N and π-π stacking interactions are found in the crystal structure and they link the molecules into a three-dimensional network.

A Three-dimensional Self-penetrating Co(Ⅱ) Coordination Polymer Containing a 2D → 3D Parallelly Polycatenated Subnet

Hydrothermal assembly of Co2＋ ion, a bis-imidazole ligand BIMB（BIMB = 1,4-bis（imidazol-1-yl）benzene） and a rigid bidentate linker 2,6-naphthalenedicarboxylic acid（H2ndc）, yields a novel three-dimensional（3D） self-penetrating coordination polymer {[Co（BIMB）（ndc）]·H2O}n（1）. Complex 1 exhibits {6~5.8} topology and contains a 2D → 3D parallel polycatenated substructure. In addition, solid-state UV-vis absorption spectra of 1 were also investigated.

A Novel Degradation Pathway of Zn(dmid)(phen)_2 in Pyridine

The light-oxidation degradation processes of Zn(dmid)(phen)_2 ( dmid = 4,5-dimercapto-l, 3-dithiole-2-one, phen = 1,10-phenanthroaline) in pyridine solvent has beenmonitored. It has been found under the light, dmid^(2-) of Zn(dmid)-(phen)_2 in pyridine solutioncould generate NCS~ and NCS^-replaces dmid^(2-) to form Zn(NCS)_2 (phen)_2 simultaneously. Thecrystal structure of Zn(NCS)_2 (phen)_2 has been determined. In the crystal of Zn(NCS)_2 (phen)_2,two NCS~ ligands are arranged in syn-configuration, and there is strong pi-pi interaction betweenthe two adjacent parallel phen.

Synthesis, Structure and Quantum Mechanical Calculations of Methyl 2-(5-((Quinolin-8-yloxy)-methyl)-1,3,4-oxadiazol-2-ylthio)-acetate

The title compound was synthesized by the base catalyzed reaction of 5-（（quinolin- 8-yloxy）methyl）-1,3,4-oxadiazole-2（3H）-thione with methyl chloroacetate. The structure was supported by the spectroscopic data and unambiguously confirmed by single-crystal X-ray diffraction studies. It crystallizes from a methanol solution in the triclinic space group Pi with unit cell dimensions a = 7.4509（9）, b = 10.2389（12）, c = 12.2299（15）A, a = 74.771（2）, β = 77.956（2）, 7 = 69.263（2）°, V = 834.98（17） A3 and Z = 2. In order to gain some valuable insights into the molecular structure, the quantum mechanical calculations were performed using both HF and time-dependent density functional theory at the B3LYP/6-31G（d,p） level. The molecular geometry from X-ray determination of the title compound in the ground state has been compared using the Hartree-Fock （HF） and density functional theory （DFT） with the 6-31G（d） basis set. The calculated results show that the DFT and HF can well reproduce the structure of the title compound. The energetic behavior of the title compound was examined using the B3LYP method with the 6-31G（d） basis set. The harmonic vibrational frequencies calculated have been compared with the experimental FTIR and FT-Raman spectra. The restricted Hartree-Fock and density functional theory-based nuclear magnetic resonance （NMR） calculation procedure was also performed, and it was used for assigning the 13C and 1H NMR chemical shifts of the title compound. Moreover, molecular electrostatic potential and thermodynamic parameters of the title compound were investigated by theoretical calculations.

Synthesis, Characterization and X-ray Crystal Structure of 2-Benzyl-7-butoxyl-9-isobutyl-1-methyl-β-carboline Bromide

2-Benzyl-7-butoxyl-9-isobutyl-1-methyl-β-carboline bromide（H-2-65） was synthesized by the reaction of Harmine with 1-iodobutane via N9-alkylation, demethyl and N2-quaternarization to obtain the new compound. The results demonstrate that H-2-65 has more remarkable anticancer activities in vitro. The results of 1H NMR, 13 C NMR, DEPT, g COSY, g HSQC, g HMBC, MS, single-crystal X-ray diffraction and elemental analysis showed that the title compound crystallizes in the triclinic system, space group P1 with a = 9.545（5）, b = 11.724（5）, c = 11.839（6） , α = 77.530（6）, β = 87.169（6）, γ = 72.823（5）o, Z = 2, V = 1235.8（10）3, Dc = 1.294 g·cm-3, F（000） = 504, the final R = 0.0453, wR = 0.1262 and S = 1.044.

Synthesis,Structure,and Optical-response Magnetic Property of a Heteroarene-azo Functionalized Mn_(19) Cluster

Metal clusters with photoswitching ligands can undergo magnetic changes under light radiation,which makes them potential optical-response magnetic-switching materials.Herein,a photoswitchable Mn-oxo cluster[Mn^(II)_(15)Mn^(III)_(4)(L)_(18)(OH)_(12)(N_(3))_(6)](ClO_(4))_(2)(C_(6)H_(5)CN)_(8),(Mn19azo,HL=1-(hydroxymethyl)-3,5-dimethyl-4-(phenyldiazenyl)-pyrazole)has been designed and synthesized to realize the photoswitching behavior.Mn19azo shows quick trans-to-cis transformation upon 365 nm light irradiation in CH2Cl2 solution and solid state as confirmed by UV-Vis spectra.After the powder sample was irradiated for 80 min,the Curie constant of Mn19azo increases by about 7%.The change of magnetic properties can be considered as the result of the change of intermolecular interactions.

Synthesis, Crystal Structure and Magnetic Properties of a 1-D Polymer, [Cu(NITpPy)_2(H_2TCB)(H_2O)]·2H_2O

A novel complex [Cu(NITpPy)_2(H_2TCB)(H_2O)]·2H_2O (NITpPy =2-(pyrid-4'-yl)-4,4,5,5-tetramethyl-1,3-dioxoimidazoline; H_2TCB = 1,5-dicarboxybenzenecarboxylic-2,4-diacid) has been synthesized and characterized by X-ray crystallography analysis. Thecrystal structure consists of infinite chains of Cu(NITpPy)_2(H_2O) units linked by H_2TCB ligands.The complex crystallizes in triclinic system with space group P1. Crystal data: a = 1.0594(2) nm, b= 1.3830(3) nm, c = 1.5551(3) nm, α = 67.75(3)°, β = 89.83(3)°, γ = 70.54(3)°. The variablemagnetic susceptibility studies lead to magnetic coupling constant values of J_1 = -11.18 cm^(-1)(Cu-Rad) and J_2 = -4.06 cm^(-1) (Cu-Cu).